Application of Miniature Specimen Test Techniques for

Nuclear Reactor Structural Materials

Post Irradiation Examination Division

Bhabha Atomic Research Centre
pritik@barc.gov.in
Why to evaluate mechanical properties of
irradiated structural materials?
Before start of
reactor operation

After few years of

reactor operation
 Microstructure Mech. Properties
Neutron on RPV Vac. & Interstitial Hardening
cluster & segregation Embrittlement

RPV
What is Miniature specimen test ?
 What is Miniature specimen test ?

 Tests, based on miniaturization or scaling down of conventional specimen size

– Miniature tensile, fatigue, impact and fracture toughness tests
 Tests, based on non-conventional techniques using existing specimen geometry
– Small punch test (TEM specimen, 10x10 mm 2 Charpy specimen cross-section),
ball indentation test (hardness test specimen)
 Tests, based on non-conventional specimen geometry
– Ring tension test, Segmented expanding mandrel test
Why to use miniature specimen testing for
irradiated structural materials?

vs

484
 miniaturization or scaling down of conventional specimen size
- Can be accommodated in less space during irradiation
- Decreases dose level
- Lesser active waste
 non-conventional techniques using existing specimen geometry
- Large number of specimens can be prepared from a given volume of material
- Used when source material is scarce
- limited space available at irradiation location
 non-conventional specimen geometry – ??
Why non-conventional specimen geometry for
irradiated structural material testing?
Why non-conventional specimen geometry for
irradiated structural material testing?

In addition to all the advantages of small size of specimen, non-conventional

specimen geometry is used because it is Relatively easy to :
- fabricate specimen remotely
- mounting or fixing specimen into machine for testing
 Outline
BACKGROUND
– Why mechanical property evaluation required for nuclear structural mat.
– Why need for miniature testing techniques
– Why need for non-conventional specimen geometry
SMALL PUNCH TEST (SPT)
– Test method details
– Evaluation and validation of correlation constants obtained for SPT
AUTOMATED BALL INDENTATION (ABI) TEST
– Test method details
– Unirradiated and irradiated material tensile properties generated using ABI
USE OF SMALL RING SPECIMENS
- Limitations of standard specimen test
- Ring Tensile Test (RTT) using ring specimens with and without gauge section
- Unirradiated and irradiated material tensile properties using simple RTT samples
- Segmented Expanding Mandrel Test (SEMT) to overcome RTT limitation
 Small Punch Test (SPT) set up

before start of test during test

 SPT specimen and load-displacement plot

Load-displacement plot
Specimen before test Tested specimen

1. Elastic region,
2. Departure from linearity (elastic-plastic transition)
3. Local bending, transitioning to a membrane stress regime
4. Membrane stress regime
5. Final failure region
Estimation and validation of correlation constants
and equations for SPT
 Estimation of correlation constants requires
Characteristic small punch load & displacement values for
yield strength, tensile strength and total elongation
Characteristic small punch force F y for yield strength

Yield Strength = α1(FYS/h02) + α2

Characteristic small punch force for tensile strength

Fm

F(0.65mm)
F(0.48mm)

Ultimate Tensile Strength = β1(FUTS/h02) + β2

Characteristic small punch displacement for total elongation

Fm

Ff Total Elongation= γ1(vm) + γ2

Total Elongation= γ1(vm - h 0) + γ2

Total Elongation= γ1(vf - h0)/ h0 + γ2

vm
vf
 Estimation of correlation constants

Tensile properties obtained for two steels from tension test

SPT of these two steels were carried out to get various

characteristic load and displacement values

Various temporary correlation constants were generated by

comparing tensile properties and SPT characeristic load-
dispalcement values using various correlations discussed
 Validation of correlation constants

SPT and tensile tests were carried out on two more steels

Earlier generated various correlation constants were used to

find tensile properties from SPT using various correlations

The correlations constants which gave minimum

percentage difference in tensile properties from tension
test and SPT test were considered as validated constants
 Useful Characteristic small punch forces and displacement

Fm

FY_int
vm

Yield Strength = α1(FY_int/h02) + α2

Ultimate Tensile Strength = β1(Fm/h02) + β2

Total Elongation= γ1(vm) + γ2

 Outline
BACKGROUND
– Why mechanical property evaluation required for nuclear structural mat.
– Why need for miniature testing techniques
– Why need for non-conventional specimen geometry
SMALL PUNCH TEST (SPT)
– Test method details
– Evaluation and validation of correlation constants obtained for SPT
AUTOMATED BALL INDENTATION (ABI) TEST
– Test method details
– Unirradiated and irradiated material tensile properties generated using ABI
USE OF SMALL RING SPECIMENS
- Limitations of standard specimen test
- Ring Tensile Test (RTT) using ring specimens with and without gauge section
- Unirradiated and irradiated material tensile properties using simple RTT samples
- Segmented Expanding Mandrel Test (SEMT) to overcome RTT limitation
 Automated Ball Indentation (ABI) Test
ABI is a nondestructive mechanical testing technique for
determining tensile and fracture toughness properties.

It is based on progressive indentation with intermediate partial

unloadings until the maximum depth (maximum strain) is
reached, and then the indenter is fully unloaded.
ABI Test plot and indentation
Automated Ball Indentation (ABI) Test
 Outline
BACKGROUND
– Why mechanical property evaluation required for nuclear structural mat.
– Why need for miniature testing techniques
– Why need for non-conventional specimen geometry
SMALL PUNCH TEST (SPT)
– Test method details
– Evaluation and validation of correlation constants obtained for SPT
AUTOMATED BALL INDENTATION (ABI) TEST
– Test method details
– Unirradiated and irradiated material tensile properties generated using ABI
USE OF SMALL RING SPECIMENS
- Limitations of standard specimen test
- Ring Tensile Test (RTT) using ring specimens with and without gauge section
- Unirradiated and irradiated material tensile properties using simple RTT samples
- Segmented Expanding Mandrel Test (SEMT) to overcome RTT limitation
Miniature and non-standard specimen tests for thin clad tube


Background: Standard mechanical test for clad tubes & limitations for irradiated clad

Key Objective: Evaluate suitable specimen test to overcome the above limitations

Technical Approach: Use of Non-standard specimen tests in the present study
A) Ring tension test on specimens with and without gauge section

As-fabricated clad

Hydrided clad with 900 wppm hydrogen
B) Ring tension test using specimens without gauge section

Irradiated clad

Irradiated clad with transient heating
C) Segmented expanding mandrel test using simple clad rings

As-fabricated clads

Clads with circumferential hydrides

Clads with radial hydrides

Summary and conclusion
 Specified mechanical test for clad
& limitations for irradiated clads

Burst Test
• Minimum specimen length for burst test is around 150mm and for a specimen
one can obtain single value of burst strength and Total Circumferential
Elongation (TCE).

Opening due to burst test

Clad tube

Limitations for irradiated clad

Defuelling
Handling large size irradiated material
Single TCE value from around 150 mm long tube piece
 Key objective

Smaller specimen that is easier to handle in hotcell

Simpler specimen type that is easier to fabricate inside hotcell

Evaluate the applicability of the specimen type for

irradiated clads
 Technical approach

(A) Use of small ring Specimens with & without gauge section

Material: Specimen:
Zircaloy-4 clad tube Ring
As-fabricated

Hydrided

 Ring Tension Test (RTT) Grip

 Technical approach (cont.)

Use of simple ring Specimen in

RTT set-up Ring specimen SEMT set-up

(B) Ring tension test (RTT) of (C) Segmented Expanding Mandrel

test (SEMT) to see effect of :
irradiated clad to see effect of :

 Hydrogen content
 Irradiation
 Hydride orientation
• Transient heating
 (A) Ring tension test of as-fabricated and hydrided clads
using specimens having gauge section and no-gauge section
 Experimental Details

As-received 900 wppm

clad hydrided clad

Hydrides Radial

Circumferentia
l

Hydriding : Gaseous charging method

Sample preparation : Slow speed cut-off wheel & EDM
Test in : Screw driven UTM
Cross-head speed : 0.5 mm/min
Test Temp. (0C) : 25, 100, 200, 300
Tensile properties of as-fabricated clads using ring
specimens with and without gauge section

Samples with gauge section

Samples without gauge section

Tensile properties of hydrides clads (900 wppm)

250C 3000C

Brittle fracture at 25 0C &

relatively ductile fracture at 300 0C
shown by both types of specimens
 Tests using Ring specimens with and without gauge section
for as-fabricated as well as hydrided clads
at different temperatures
have shown comparable results

Simple ring without any gauge section can be used for irradiated clad tests

However, ring tension test is giving around 30% elongation compared to

around 15% TCE observed in Burst test of as-fabricated clads
(B) Ring tension test of irradiated clads
 Sample preparation inside hotcell

Punching handle
Fuel pin

Sample holder
Sample cutting Defuelling

Clad ring Clad ring

manipulator finger
Ring width measurement
 Ring tension test fixture

Clad ring

Transient heating: vacuum furnace

Test in : Screw driven UTM Heating temp. : 400, 500, 600, 7000C
Time at high temp.: 2 min
Cross-head speed: 0.5 mm/min Post-heating : water quenching
 Effect of Irradiation on as-fabricated clad &
Transient heating effect on irradiated clad

Irradiation increased strength by 45% &

decreased ductility by 75%

Transient heating at 400 0C for 2 min showed no change in properties

Transient heating at 600 0C for 2 min led to complete recovery of properties
 Effect of irradiation and transient heating effect
could be determined using simple rings in ring tension test.

Simple ring without any gauge section can be used for irradiated clad tests

However, uniaxial loading and smaller gauge length in ring tension test
as compared to bi-axial loading and large deforming length in burst test
may give different elongation values
(C) Segmented expanding mandrel test of clads
Segmented expanding mandrel test of clads

Upper cone

Mandrel
segments

Ring sample
 Different stages of test in
progress
Segmented
mandrel

Ring sample
Effect of Hydride orientation on as-fabricated clad

Hydriding (200 wppm) : Electrolytic method

Sample preparation : slow speed cut-off wheel
Hydride re-orientation : Thermo-mechanical treatment
Test in : Screw driven UTM
Cross-head speed : 0.5 mm/min

Clad condition Diametral strain (%)

As-fabricated : 12

Hydrided (cirum.) : 10
(200wppm)

Hydrided (Radial) : 1.8

(200wppm)
 Specimens of Segmented expanding mandrel test

Clads with Circumferential hydrides Clads with Radial hydrides

Radial
Radial
Circumferentia Circumferential
l

Clads with circumferential hydrides have shown 450 shear fracture

Clads with radial hydrides have shown flat brittle fracture
 Results of Burst test(BT), RTT and SEMT

As-compared to RTT the results of SEMT are relatively closer to BT result

Difference between RTT & SEMT decreased with increased brittleness
 Summary and conclusion on RTT
Mechanical tests were carried out using non-standard specimens of Zircaloy-4 clad.
The main findings are:

 Ring specimens with and without gauge section showed comparable results for as-
fabricated as well as for hydrided clads
 Simple ring sample without gauge section can be used for evaluating
tensile properties of irradiated clads
 Simple rings have the advantage to easier fabrication, easier handling,
easier test

 Ring tension test (RTT) of irradiated clad using simple rings without gauge section
showed that
 Irradiation led to 45% increase in strength and 75% decrease in ductility
 Transient heating at 4000C has no effect on tensile properties
 Transient heating at 6000C led to complete recovery of tensile properties
 Summary and conclusion on RTT and SEMT

 Segmented expanding mandrel (SEMT) test using ring specimen without any gauge
section has shown the effect of hydride (200wppm) orientation on clad ductility
 Circumferential hydrides not much effect on diametral strain
 Radial hydrides have shown drastic brittleness & <2% diametrail strain

 BT, RTT and SEMT results have been compared.

 For clads with 200 wppm hydrogen, RTT showed higher elongation
compared to BT
 Total circumferential elongation from SEMT and BT are quite comparable
 Difference between RTT & SEMT decreased with increased brittleness

For irradiated clad simple rings around 3 mm width can give an estimate
of effect of irradiation and hydrides on mechanical properties of clad
 Outline
BACKGROUND
– Why mechanical property evaluation required for nuclear structural mat.
– Why need for miniature testing techniques
– Why need for non-conventional specimen geometry
SMALL PUNCH TEST (SPT)
– Test method details
– Evaluation and validation of correlation constants obtained for SPT
AUTOMATED BALL INDENTATION (ABI) TEST
– Test method details
– Unirradiated and irradiated material tensile properties generated using ABI
USE OF SMALL RING SPECIMENS
- Limitations of standard specimen test
- Ring Tensile Test (RTT) using ring specimens with and without gauge section
- Unirradiated and irradiated material tensile properties using simple RTT samples
- Segmented Expanding Mandrel Test (SEMT) to overcome RTT limitation
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